CN105129797A - Preparation method of ammoniation-activation plant activated carbon - Google Patents
Preparation method of ammoniation-activation plant activated carbon Download PDFInfo
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- CN105129797A CN105129797A CN201510428036.4A CN201510428036A CN105129797A CN 105129797 A CN105129797 A CN 105129797A CN 201510428036 A CN201510428036 A CN 201510428036A CN 105129797 A CN105129797 A CN 105129797A
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Abstract
The invention discloses a preparation method of ammoniation-activation plant activated carbon, which includes following steps: (1) performing ammoniation treatment to plant raw materials with ammoniation reagents, such as urea, ammonium bicarbonate, ammonia water and the like, to obtain an ammoniated raw material; (2) mixing the ammoniated raw material with an activating agent uniformly and performing impregnation for 2-12 h, wherein the mass ratio of the ammoniated raw material to the activating agent is 1:0.5-2.0; (3) performing carbonization and activation to the impregnated raw material at 300-800 DEG C for 30-60 min to obtain activated carbon; and (4) washing and drying the activated carbon to obtain the product. The preparation method is low in production cost and simple in production process. The activated carbon is high in specific surface area and abundant in functional groups when compared with activated carbon prepared through a conventional method.
Description
Technical field
The invention belongs to field of functional materials, particularly relate to the preparation method of a kind of ammonification-activation phyteral gac.
Background technology
Gac, as a kind of common sorbent material, is widely used in absorption and the removal of objectionable impurities in gas phase and liquid phase.The ability of its adsorb pollutants mainly comes from flourishing aperture structure and abundant functional group acidic functionality and basic functionalities such as () carboxyl, lactone group, phenolic hydroxyl groups.In recent years, in order to meet the market requirement that constantly expands and the human consumer requirement to more high efficiency active carbon, the producer improves its physicochemical property and absorption property usually through methods such as modifications.A lot of research proves, phyteral gac has the advantages such as quality is high, performance is good.So phyteral raw material obtains a large amount of popularizations, application in gac preparation field.In phyteral gac traditional preparation methods, be direct impregnation after charcoal precursor is pulverized, activation mostly, the defects such as cause activator to flood insufficient, utilization ratio is low, and dipping time is long, and activation temperature is high, and gac specific surface area is low, and number of functional groups is few.For the deficiency that traditional method exists, propose the preparation method of phyteral raw material ammoniated treatment.
Through retrieval, the technique that ammonification-activation method prepares phyteral gac is a technological gap at present.
Summary of the invention
The present invention overcomes the weak point that traditional method prepares gac, provides the processing method of a kind of ammonification-activation phyteral gac.Phyteral raw material is first carried out ammoniated treatment preparing in gac process by this method, then carries out carbonization-activation.Gac prepared by this method has higher specific surface area and flourishing surface functional group.
Technical scheme of the present invention is as follows:
A kind of preparation method of ammonification-activation phyteral gac, comprises the following steps:
(1) adopt the aminating agent such as urea, bicarbonate of ammonia or ammoniacal liquor to carry out ammoniated treatment to phyteral raw material, obtain the raw material after ammonification;
(2) raw material after ammonification in step (1) and activator are mixed, at 20 ~ 30 DEG C of dipping 2 ~ 12h, the raw material after described ammonification and the mass ratio of activator are 1:0.5 ~ 2.0;
(3) the raw material carbonization-activation 30 ~ 60min at 300 ~ 800 DEG C after dipping, obtains gac;
(4) by washing active carbon, drying, product is obtained.
Before phyteral raw material carries out ammoniated treatment, carry out pre-treatment to phyteral raw material, pretreatment process is: washed by phyteral raw material, dry, be crushed to 20 ~ 40 orders; Carrying out pretreated benefit is: in order to make the process of ammoniated treatment more abundant, aminating agent and phyteral raw material reaction contact area are larger, to reduce the ammonification time, raise the efficiency.
In step (1), described phyteral raw material is one or more mixing of reed, giantreed or great Ye reed, through verification experimental verification, after above-mentioned three kind of plant raw material reeds, giantreed or great Ye reed adopt ammonification-activation treatment, effect is best, has higher specific surface area and flourishing functional group.
In step (1), when aminating agent be urea or bicarbonate of ammonia time, the concrete grammar of ammoniated treatment is: be that 0.03 ~ 0.08:1 with urea or bicarbonate of ammonia mix according to urea or bicarbonate of ammonia with the mass ratio of phyteral raw material by phyteral raw material, be dissolved in water, sealing, keep 1 ~ 6h at 90 ~ 100 DEG C, preferable temperature is 100 DEG C.
Through experimental demonstration and analysis, when the mass ratio obtaining urea or bicarbonate of ammonia and phyteral raw material is 0.03 ~ 0.08:1, the effect of ammonification and efficiency are all best, when ratio is higher, not only waste aminating agent, contaminate environment, and also can cause trouble during subsequent wash; When ratio is lower, ammonification is not embodied fully, and gac does not obtain higher specific surface area and flourishing functional group.
In step (1), when aminating agent is ammoniacal liquor, the concrete grammar of ammoniated treatment is: be that 0.01 ~ 0.05:1 mixes with ammoniacal liquor by phyteral raw material according to ammoniacal liquor and the mass ratio of phyteral raw material, sealing, keep 5 ~ 14d at 18 ~ 30 DEG C, preferable temperature is 25 DEG C.Preferably, the mass concentration of ammoniacal liquor is 3 ~ 15%.
Through experimental demonstration and analysis, when the mass ratio obtaining ammoniacal liquor and phyteral raw material is 0.01 ~ 0.05:1, the effect of ammonification and efficiency are all best, when ratio is higher, not only waste aminating agent, contaminate environment, and also can cause trouble during subsequent wash; When ratio is lower, ammonification is not embodied fully, and gac does not obtain higher specific surface area and flourishing functional group.
In step (2), activator is phosphoric acid solution or potassium hydroxide, and the massfraction of described phosphoric acid solution is 30 ~ 55%.
In step (2), preferably, described dipping time is 2 ~ 8h.
According to the situation dipping 2 ~ 8h of the phyteral raw material after ammonification, the phyteral raw material after this dipping time can make ammonification fully activates, and the time is too short, and not exclusively, dipping effect is undesirable for dipping; Overlong time, loses time, lowers efficiency.
In step (3), preferably, described temperature is 300 ~ 450 DEG C, and the described time is 30 ~ 60min.After ammoniated treatment, (carbonization temperature of the phyteral method for preparation of active carbon of non-ammonification is 500 ~ 900 DEG C significantly can to reduce carbonization temperature and time, carbonization time is 1 ~ 4h), the standard of the carbon content of gac can be met through this carbonization temperature of verification experimental verification and time.
In step (4), washing active carbon to pH value is stabilized in about 7.0 and carries out drying again, reason is: washing active carbon is to acid or alkaline words, the reaction of gac environment may be affected, such as washing active carbon, to alkalescence, so may react with the acidic substance in gac environment.
Ammonification is for phyteral raw material, the chemical bonds between xylogen and polysaccharide can be destroyed, make Mierocrystalline cellulose, hemicellulose and lignin separation, insoluble xylogen is become more molten hydroxyl xylogen, crystalline cellulose becomes amorphous cellulose, causes cell expansion, makes phyteral raw material mix become loose; Further, in ammonifying process, in phyteral raw material, the content of crude protein significantly improves, and can improve amido functional group quantity.In process prepared by phyteral gac, phyteral raw material is carried out ammoniated treatment, effectively can strengthen dipping effect, improve the specific surface area of gac, increase the quantity of gac functional group.
The present invention has following advantage compared with traditional preparation method:
(1) raw material uses the phyteral raw materials such as stalk, has widely distributed, advantage with low cost.
(2) aminating agent consumption is little, and pollution on the environment is little.
(3) due to ammonification, activator usage quantity reduces, and activation temperature reduces, cost-saving, reduces energy consumption, decreasing pollution.
(4) production cost is low, and production technique is simple, and obtained gac has high specific surface area and more rich functional group relative to traditional method.
(5) through great many of experiments and analysis, the adsorption effect of activated carbon in water that preparation method of the present invention obtains is better than the adsorption effect of the gac that common method prepares.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
Reed washed, dries, be crushed to 40 orders; Inject and be equivalent to ammoniacal liquor and its mixing that reed dry matter weight mass concentration is 3%, sealing, keeps 7d to carry out ammoniated treatment at 25 DEG C; By the reed powder after ammonification and 45wt.% phosphoric acid solution 1:1 room temperature immersion 5h in mass ratio; Macerate proceeds to crucible and is built in retort furnace, and at 300 DEG C, carbonization-activation 40min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.The gac specific surface area that gained gac is prepared compared with traditional method reference examples 1 improves 20%, and total number of functional groups improves 46%.
Reference examples 1
Reed washed, dries, be crushed to 40 orders, by reed powder and 45wt.% phosphoric acid solution 1:2 dipping 10h in mass ratio; Macerate proceeds to crucible and is built in retort furnace, and at 500 DEG C, carbonization-activation 60min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.
Embodiment 2
Reed washed, dries, be crushed to 40 orders; Get the urea being equivalent to reed dry matter weight 7%, every 10g reed dry matter weight adds 2ml water dissolution, and aqueous solution of urea and reed powder mix, and sealing, keeps 2h, carry out ammoniated treatment at 100 DEG C; By the reed powder after ammonification and potassium hydroxide in mass ratio 1:2 at 30 DEG C of dipping 2h; Macerate proceeds to nickel crucible and is built in retort furnace, and at 650 DEG C, carbonization-activation 60min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.Its specific surface area comparatively traditional method reference examples 2 improves 15%, and surface functional group quantity improves 50%.
Reference examples 2
Reed washed, dries, be crushed to 40 orders, by reed powder and potassium hydroxide 1:2 dipping 8h in mass ratio; Macerate proceeds to crucible and is built in retort furnace, and at 900 DEG C, carbonization-activation 120min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.
Embodiment 3
Reed washed, dries, be crushed to 40 orders; Get the bicarbonate of ammonia of reed powder dry matter weight 5%, every 10g reed powder dry matter weight adds 2ml water dissolution, and ammonium bicarbonate aqueous solution and reed powder mix, and sealing, keeps 4h, carry out ammoniated treatment at 100 DEG C; By reed powder after ammonification and 45wt.% phosphoric acid solution in mass ratio 1:1.5 at 20 DEG C of dipping 8h; Macerate proceeds to crucible and is built in retort furnace, and at 400 DEG C, carbonization-activation 60min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.Its specific surface area comparatively traditional method reference examples 3 improves 15%, and number of functional groups improves 18%.
Reference examples 3
Reed washed, dries, be crushed to 40 orders, by reed powder and 45wt.% phosphoric acid solution 1:1.5 dipping 8h in mass ratio; Macerate proceeds to crucible and is built in retort furnace, and at 650 DEG C, carbonization-activation 90min, naturally cools to room temperature; Be about 7 by gained gac deionized water wash to pH, solid-liquid separation, oven dry.
Table 1: gac specific surface area, aperture parameters and number of functional groups.
Through test, giantreed, great Ye reed obtain effect good equally.
Embodiment 4
Utilize embodiment 1 and the obtained activated carbon application of comparative example 1 in sanitary sewage, wastewater from chemical industry and pharmacy waste water, three kinds of sewage experimental result before and after charcoal absorption is in table 2.
The adsorption effect of activated carbon in water of table 2 embodiment 1 and comparative example 1
Residual organic matter in waste water, residual suspended substance etc. realize being separated of pollutent and water body by the filtration of gac, absorption, and table 2 can find out that the adsorption effect of the gac adopting the method for embodiment 1 to prepare obviously is better than the adsorption effect of the gac of comparative example 1 intuitively.
Claims (10)
1. a preparation method for ammonification-activation phyteral gac, is characterized in that, comprise the following steps:
(1) adopt urea, bicarbonate of ammonia or ammoniacal liquor aminating agent to carry out ammoniated treatment to phyteral raw material, obtain the raw material after ammonification;
(2) raw material after the ammonification in step (1) and activator are mixed, 20 ~ 30
oc floods 2 ~ 12h, and the raw material after described ammonification and the mass ratio of activator are 1:0.5 ~ 2.0;
(3) raw material after dipping is 300 ~ 800
ounder C, carbonization-activation 30 ~ 60min, obtains gac;
(4) by washing active carbon, drying, product is obtained.
2. preparation method as claimed in claim 1, it is characterized in that: before phyteral raw material carries out ammoniated treatment, carry out pre-treatment to phyteral raw material, pretreatment process is: phyteral raw material is washed, dries, pulverized, and is crushed to 20 ~ 40 orders.
3. preparation method as claimed in claim 1, is characterized in that: in step (1), and described phyteral raw material is one or more mixing of reed, giantreed or great Ye reed.
4. preparation method as claimed in claim 1, it is characterized in that: in step (1), when aminating agent be urea or bicarbonate of ammonia time, the concrete grammar of ammoniated treatment is: be that 0.03 ~ 0.08:1 with urea or bicarbonate of ammonia mix according to urea or bicarbonate of ammonia with the mass ratio of phyteral raw material by phyteral raw material, be dissolved in water, sealing, 90 ~ 100
oc keeps 1 ~ 6h.
5. preparation method as claimed in claim 1, it is characterized in that: in step (1), when aminating agent is ammoniacal liquor, the concrete grammar of ammoniated treatment is: be that 0.01 ~ 0.05:1 mixes with ammoniacal liquor by phyteral raw material according to ammoniacal liquor and the mass ratio of phyteral raw material, sealing, 18 ~ 30
oc keeps 5 ~ 14d.
6. preparation method as claimed in claim 5, is characterized in that: the mass concentration of described ammoniacal liquor is 3 ~ 15%.
7. preparation method as claimed in claim 1, it is characterized in that: in step (2), activator is phosphoric acid solution or potassium hydroxide.
8. preparation method as claimed in claim 1, it is characterized in that: in step (2), described dipping time is 2 ~ 8h.
9. preparation method as claimed in claim 1, it is characterized in that: in step (3), described temperature is 350 ~ 450
oc, the described time is 40 ~ 60min.
10. the preparation method as described in as arbitrary in claim 1 ~ 9, is characterized in that: in step (4), washing active carbon to pH value is stabilized in about 7.0 and carries out drying again.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219539A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon |
| CN106927461A (en) * | 2017-03-28 | 2017-07-07 | 南平元力活性炭有限公司 | A kind of high-capacity and long-life activated carbon for super capacitors production technology |
| CN107010624A (en) * | 2017-04-24 | 2017-08-04 | 安徽大学 | A kind of nitrogen, boron for electrode of super capacitor adulterates porous charcoal and preparation method thereof |
| CN107128918A (en) * | 2017-05-26 | 2017-09-05 | 桂林电子科技大学 | A kind of preparation and its application of N doping porous active Carbon Materials |
| CN108467036A (en) * | 2018-05-22 | 2018-08-31 | 吉林化工学院 | A kind of desiliconization rice husk matrix activated carbon and its preparation method and application |
| CN108821282A (en) * | 2018-08-24 | 2018-11-16 | 山东大学 | The method that the modified sedge matrix activated carbon of shrimp chaff prepares the active carbon of high nitrogen-containing functional group |
| JP2019517982A (en) * | 2016-05-30 | 2019-06-27 | アドベン インダストリーズ, インコーポレイテッドAdven Industries, Inc. | Activated carbon having high surface area and method for producing the same |
| CN110156007A (en) * | 2019-06-20 | 2019-08-23 | 运城学院 | A kind of preparation method of giantreed active carbon |
| CN110541016A (en) * | 2019-09-10 | 2019-12-06 | 贵州好菇粮农业科技有限公司 | Extraction and purification method of lentinan |
| CN111253960A (en) * | 2020-02-13 | 2020-06-09 | 山东大学 | Straw biochar and low-temperature preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121514A (en) * | 2007-07-27 | 2008-02-13 | 邹炎 | Water purification active carbon prepared from vegetal castoff and preparation method thereof |
| CN104445141A (en) * | 2014-11-07 | 2015-03-25 | 同济大学 | Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof |
| CN104495837A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Sargassum-based activated carbon and preparation method and application thereof |
-
2015
- 2015-07-20 CN CN201510428036.4A patent/CN105129797B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121514A (en) * | 2007-07-27 | 2008-02-13 | 邹炎 | Water purification active carbon prepared from vegetal castoff and preparation method thereof |
| CN104445141A (en) * | 2014-11-07 | 2015-03-25 | 同济大学 | Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof |
| CN104495837A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Sargassum-based activated carbon and preparation method and application thereof |
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| JP2019517982A (en) * | 2016-05-30 | 2019-06-27 | アドベン インダストリーズ, インコーポレイテッドAdven Industries, Inc. | Activated carbon having high surface area and method for producing the same |
| US11124418B2 (en) | 2016-05-30 | 2021-09-21 | Adven Industries, Inc. | Activated carbons with high surface areas and methods of making same |
| CN106219539A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon |
| CN106927461A (en) * | 2017-03-28 | 2017-07-07 | 南平元力活性炭有限公司 | A kind of high-capacity and long-life activated carbon for super capacitors production technology |
| CN107010624A (en) * | 2017-04-24 | 2017-08-04 | 安徽大学 | A kind of nitrogen, boron for electrode of super capacitor adulterates porous charcoal and preparation method thereof |
| CN107128918A (en) * | 2017-05-26 | 2017-09-05 | 桂林电子科技大学 | A kind of preparation and its application of N doping porous active Carbon Materials |
| CN108467036A (en) * | 2018-05-22 | 2018-08-31 | 吉林化工学院 | A kind of desiliconization rice husk matrix activated carbon and its preparation method and application |
| CN108467036B (en) * | 2018-05-22 | 2021-10-15 | 吉林化工学院 | Desiliconized rice hull-based activated carbon and preparation method and application thereof |
| CN108821282A (en) * | 2018-08-24 | 2018-11-16 | 山东大学 | The method that the modified sedge matrix activated carbon of shrimp chaff prepares the active carbon of high nitrogen-containing functional group |
| CN108821282B (en) * | 2018-08-24 | 2020-08-25 | 山东大学 | Method for preparing active carbon with high nitrogen-containing functional groups by using shrimp bran modified Cyperaceae plant-based active carbon |
| CN110156007A (en) * | 2019-06-20 | 2019-08-23 | 运城学院 | A kind of preparation method of giantreed active carbon |
| CN110541016A (en) * | 2019-09-10 | 2019-12-06 | 贵州好菇粮农业科技有限公司 | Extraction and purification method of lentinan |
| CN111253960A (en) * | 2020-02-13 | 2020-06-09 | 山东大学 | Straw biochar and low-temperature preparation method thereof |
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